CN101244933B - Preparation method of sheet bismuth sodium titanate templated grain - Google Patents
Preparation method of sheet bismuth sodium titanate templated grain Download PDFInfo
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- CN101244933B CN101244933B CN 200810034763 CN200810034763A CN101244933B CN 101244933 B CN101244933 B CN 101244933B CN 200810034763 CN200810034763 CN 200810034763 CN 200810034763 A CN200810034763 A CN 200810034763A CN 101244933 B CN101244933 B CN 101244933B
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Abstract
The invention relates to a schistic bismuth sodium titanate template crystal grain and a preparation method thereof, belonging to the preparation field of textured non-lead piezoelectric ceramic template crystal grain, the chemical formula of the template grains is Na0.5Bi0.5TiO3, the appearance of the crystal grain is schistic, the radial length is 5 to 15Mum, the thickness is 0.5 to 1.0Mum, the crystal grain has large aspect ratio and strong orientation, which is an ideal template crystal grain. The crystal grain adopts schistic Bi4Ti3O12 as a precursor which is synthesized by molten salt method, in the molten salt system of NaCl, the crystal grain can have topological chemical reaction with Na2CO3, TiO2 so as to produce schistic polycrystalline Na0.5Bi0.5TiO3 template crystal grain and the crystal grain can be regarded as the template for various textured bismuth sodium tianate non-lead piezoelectric ceramics, which has positive effect for improving the density, the orientation and piezoelectric properties of textured bismuth sodium tianate non-lead piezoelectric ceramics.
Description
Technical field
The present invention relates to a kind of sheet bismuth sodium titanate mould plate grain and preparation method thereof, belong to texturing leadless piezoelectric ceramics template grains preparation field.
Background technology
Ferroelectric piezoelectric ceramics and device thereof all have widely in industry, the product for civilian use and military affairs and use, and are that a class is important, irreplaceable, the High-tech Material that international competition is very fierce.At present, piezoelectric ceramics commonly used is leaded pottery mostly, and such as PZT, PMN-PT etc., these lead base piezoelectric ceramics have shown very excellent performance near its accurate homotype phase boundary.But plumbous toxicity and environmental pollution thereof have caused more and more to human society and have seriously influenced.In recent years, development and eco-friendly leadless piezoelectric ceramics have attracted the concern of increasing researcher.
In numerous leadless piezoelectric ceramics systems, bismuth-sodium titanate Na
0.5Bi
0.5TiO
3(NBT) strong with its ferroelectricity, the advantage that Curie temperature is high is considered to most important one of the candidate material that replaces the lead base piezoelectric ceramics that is expected.People have done large quantity research by doping vario-property, but its performance still has gap with leaded ceramic phase ratio.Result of study in recent years shows, optimizes microstructure of ceramics by texturing, but the piezoelectric property of Effective Raise pottery,
The texturing technology refers to by technology controlling and process, and the ceramic crystalline grain of script random orientation is aligned, and makes it to have the performance near monocrystalline.Traditional doping vario-property although can improve lead-free ceramics piezoelectric property at room temperature, has also reduced Curie temperature simultaneously, thereby has limited the application of material.The texturing technology can keep the composition of material constant, is a kind of structurally-modified, compares with doping vario-property, has advantages of not change ceramic Curie temperature.In addition, textured ceramics is forming handiness, is better than especially on homogeneity and the production cost with the monocrystal material that forms.
At present, the more ceramic texturing technology of research has template grain growth (TGG) technology and reaction template grain growing (RTGG) technology.In these two kinds of methods, preparing anisotropic template grains is a key step.For NBT base pottery, the SrTiO of sheet
3(ST) and Bi
4Ti
3O
12(BiT) be two kinds of template grains commonly using.Although the texturing NBT that makes take ST as template base pottery has higher orientation degree, because the existence of ST paraelectric phase can cause ceramic Curie temperature reduction, piezoelectric property to worsen.And with BiT during as template, owing to used a large amount of BiT template grains, thus hindered the densification process of textured ceramics, be difficult to obtain simultaneously high-orientation and highdensity textured ceramics.
For NBT base pottery, best mould material is the NBT powder with sheet-like morphology.But NBT belongs to perovskite structure, has higher symmetry, and crystal grain easily develops into cubic when spontaneous growth, thereby is difficult to obtain anisotropic pattern.Therefore, in the prior art, be difficult to make the NBT template grains with sheet-like morphology feature.
Summary of the invention
The object of the invention is to the synthetic sheet Bi of molten-salt growth method
4Ti
3O
12As presoma, in the melting salt system of NaCl, with Na
2CO
3, TiO
2Topochemical reaction occurs, and can make the polycrystalline Na with flaky crystalline grain pattern
0.5Bi
0.5TiO
3Powder.This powder grain orientation is obvious, and radical length is 5～15 μ m, and thickness is 0.5～1.0 μ m, has large the ratio of width to height, is a kind of desirable template grains that is suitable for TGG and RTGG technology.The present invention has successfully solved sheet Na
0.5Bi
0.5TiO
3The difficult problem that template grains is difficult to prepare.
Purpose of the present invention can realize by the following technical solutions:
(1) adopts the in the past molten-salt growth method synthesizing flaky Bi of report
4Ti
3O
12As presoma; Be specially and adopt synthesizing flaky Bi under the eutectic molten salt system high temperature of NaCl/KCl
4Ti
3O
12Step can comprise: with Bi
2O
3And TiO
2Be material powder, press chemical formula Bi
4Ti
3O
12Batching, again with etc. eutectic fused salt warp (total mass of powder and fused salt and the ZrO in ethanol (total mass with the mass ratio 1: 0.4～0.6 of ethanol) of NaCl/KCl (mol ratio 1: 1) of quality
2The mass ratio of ball 1: 1～3) ball milling mixes, and after drying, the screening, is warming up to 950～1100 ℃ with the temperature rise rate of 3～20 ℃/min, and 0.5-6h is with the synthesizing flaky presoma in insulation;
(2) the sheet presoma that step (1) is synthetic through washing, filtration, oven dry, adds Na
2CO
3, TiO
2Powder is pressed chemical formula Na
0.5Bi
0.5TiO
3Batching, and with etc. the NaCl fused salt of quality warp (total mass of powder and fused salt and ZrO in ethanol (total mass of powder and fused salt and the mass ratio of ethanol 1: 0.4～0.6)
2The mass ratio of ball 1: 1～3) ball milling mixes, and after the oven dry, is warming up to 1000～1100 ℃, insulation 1-6h with the high temperature rise rate of 3-20 ℃/min.
(3) the synthetic powder of step (2) through washing, filtration, oven dry, can obtain required sheet Na
0.5Bi
0.5TiO
3Template grains.
Adopting the present invention successfully to prepare the chemical formula with flaky crystalline grain pattern characteristics is Na
0.5Bi
0.5TiO
3Template grains.The XRD analysis of powder shows, prepared powder has stronger orientation;
Sem analysis shows, sheet bismuth sodium titanate mould plate grain in the form of sheets, radical length is 5～15 μ m, thickness is 0.5～1.0 μ m, having large the ratio of width to height, is a kind of desirable template grain growth (TGG) technology that is suitable for and the template grains of reaction template grain growing (RTGG) technology application.
Adopt the prepared bismuth-sodium titanate powder of the present invention program, can be used as the template grains of the texturing bismuth-sodium titanate base lead-free piezoelectric ceramic of various compositions, for the density, orientation degree and the piezoelectric property that improve the texturing bismuth-sodium titanate base lead-free piezoelectric ceramic positive effect is arranged, thereby be conducive to promote the development process that leadless piezoelectric ceramics replaces the lead base piezoelectric ceramics.
Compare with existing template grains technology of preparing, the present invention has following characteristics and advantage:
1, the present invention has selected bismuth laminated Bi first
4Ti
3O
12As presoma, its crystal grain has stronger orientation and larger the ratio of width to height.
2, the prepared Na of the present invention
0.5Bi
0.5TiO
3Powder, its crystal grain has the pattern of sheet, and large the ratio of width to height and very strong orientation, radical length are 5～15 μ m, and thickness is 0.5～1.0 μ m, and moderate dimensions is a kind of desirable template grains.
3, the selected cost of material of the present invention is cheap, the preparation method is simple, is easy to promote.
Description of drawings
Fig. 1 is Bi
4Ti
3O
12The XRD figure spectrum of presoma.(a) Bi
4Ti
3O
12The XRD figure spectrum of standard P DF card (00-056-0814); (b) the prepared sheet Bi of the present invention
4Ti
3O
12(1100 ℃, XRD figure spectrum 0.5h).
Fig. 2 is Bi
4Ti
3O
12(1100 ℃, 0.5h) the SEM photo of presoma.
Fig. 3 is Na
0.5Bi
0.5TiO
3The XRD figure spectrum of powder.(a) Na
0.5Bi
0.5TiO
3The XRD figure spectrum of standard P DF card (01-070-9850); (b) the prepared sheet Na of the present invention
0.5Bi
0.5TiO
3(1100 ℃, XRD figure spectrum 2h); (c) the prepared sheet Na of the present invention
0.5Bi
0.5TiO
3(1100 ℃, XRD figure spectrum 4h).
Fig. 4 is Na
0.5Bi
0.5TiO
3Powder (1100 ℃, SEM photo 2h).
Fig. 5 is Na
0.5Bi
0.5TiO
3Powder (1100 ℃, SEM photo 4h).
Embodiment
Below in the mode of specific embodiment the present invention is described but is not limited only to embodiment.
Embodiment 1
1, precursor synthesis: according to Bi
4Ti
3O
12Reaction equation calculate, accurately take by weighing Bi
2O
3(purity: 99.9%) 7.9621g, TiO
2(purity: 99.8%) 2.0500g, NaCl (purity: 100%) 4.4053g and KCl (purity: 99%) 5.6634g, each raw material and ethanol 10ml, ZrO
2Behind the ball 40g mixing and ball milling 24h, be transferred in the Glass Containers and dry.Dried material powder contains Al after screening
2O
3Crucible, add a cover, 1100 ℃ of synthetic 0.5h in High Temperature Furnaces Heating Apparatus, temperature rise rate is 5 ℃/min.
2, presoma filters: with synthetic Bi
4Ti
3O
12Presoma is pulverized, through ultra-sonic dispersion, 10 deionized water wash, to remove NaCl and KCl fused salt wherein.Fig. 1 is prepared Bi
4Ti
3O
12The XRD figure spectrum of presoma, as we can see from the figure, the intensity of its (001) diffraction peak strengthens to some extent, has stronger orientation; Its SEM photo as shown in Figure 2, as can be seen from the figure, Bi
4Ti
3O
12The crystal grain of presoma in the form of sheets, its radical length is 5～15 μ m, thickness is 0.2～0.5 μ m, has large the ratio of width to height.
3, sheet Na
0.5Bi
0.5TiO
3Synthetic: according to Na
0.5Bi
0.5TiO
3Chemical equation calculate accurate weighing Na
2CO
3(purity: 99.95%) 1.2512g, TiO
2(purity: 99.8%) 2.3616g, NaCl (purity: 100%) 10.5248g, each raw material and ethanol 7ml, ZrO
2Behind the ball 28g mixing and ball milling 20h, the accurate synthetic Bi of weighing again
4Ti
3O
12Presoma 6.9120g, and add ethanol 3ml, ZrO
2Ball 12g is transferred in the Glass Containers and dries after continuing ball milling 4h.Dried material powder contains Al after screening
2O
3Crucible, add a cover, 1100 ℃ of synthetic 2h in High Temperature Furnaces Heating Apparatus, temperature rise rate is 10 ℃/min.
4, sheet Na
0.5Bi
0.5TiO
3Filter: with synthetic Na
0.5Bi
0.5TiO
3Pulverize, through ultra-sonic dispersion, 10 deionized water wash, to remove NaCl fused salt wherein.Prepared Na
0.5Bi
0.5TiO
3Powder, its XRD figure are composed shown in Fig. 3 (b), as we can see from the figure, and sheet Na
0.5Bi
0.5TiO
3The intensity of (001) diffraction peak greatly strengthen, have stronger orientation; The SEM photo as shown in Figure 4, as we can see from the figure, most Na
0.5Bi
0.5TiO
3Powder, its crystal grain presents the pattern of sheet, and radical length is 5～15 μ m, but still has small portion crystal grain for waiting axle carefully brilliant, and crystallization is incomplete.
Embodiment 2
1, precursor synthesis: according to Bi
4Ti
3O
12Reaction equation calculate accurate weighing Bi
2O
3(purity: 99.9%) 7.9621g, TiO
2(purity: 99.8%) 2.0501g, NaCl (purity: 100%) 4.4055g and KCl (purity: 99%) 5.6635g, each raw material and ethanol 7ml, ZrO
2Behind the ball 40g mixing and ball milling 24h, be transferred in the Glass Containers and dry.Dried material powder contains Al after screening
2O
3Crucible, add a cover, 1100 ℃ of synthetic 0.5h in High Temperature Furnaces Heating Apparatus, temperature rise rate is 5 ℃/min.
2, presoma filters: with synthetic Bi
4Ti
3O
12Presoma is pulverized, through ultra-sonic dispersion, 10 deionized water wash, to remove NaCl and KCl fused salt wherein.Prepared Bi
4Ti
3O
12Presoma, its XRD figure is composed as shown in Figure 1, and as we can see from the figure, the intensity of its (001) diffraction peak strengthens to some extent, has stronger orientation; The SEM photo as shown in Figure 2, as can be seen from the figure, Bi
4Ti
3O
12The crystal grain of presoma in the form of sheets, its radical length is 5～15 μ m, thickness is 0.2～0.5 μ m, has large the ratio of width to height.
3, sheet Na
0.5Bi
0.5TiO
3Synthetic: according to Na
0.5Bi
0.5TiO
3Chemical equation, accurate weighing Na
2CO
3(purity: 99.95%) 1.0010g, TiO
2(purity: 99.8%) 1.8893g, NaCl (purity: 100%) 8.4200g, each raw material and ethanol 6ml, ZrO
2Behind the ball 23g mixing and ball milling 20h, the accurate synthetic Bi of weighing again
4Ti
3O
12Presoma 5.5296g, and add ethanol 3ml, ZrO
2Ball 11g is transferred in the Glass Containers and dries after continuing ball milling 4h.Dried material powder contains Al after screening
2O
3Crucible, add a cover, 1100 ℃ of synthetic 4h in High Temperature Furnaces Heating Apparatus, temperature rise rate is 10 ℃/min.
4, sheet Na
0.5Bi
0.5TiO
3Filter: with synthetic Na
0.5Bi
0.5TiO
3Pulverize, through ultra-sonic dispersion, 10 deionized water wash, to remove NaCl fused salt wherein.Prepared Na
0.5Bi
0.5TiO
3Powder, its XRD figure are composed shown in Fig. 3 (c), as we can see from the figure, behind the prolongation sintering time, sheet Na
0.5Bi
0.5TiO
3The intensity of (001) diffraction peak further strengthen, preferred orientation is more obvious, has very strong orientation; The SEM photo is compared with Fig. 4 as shown in Figure 5, this Na
0.5Bi
0.5TiO
3The powder crystallization is more complete, and crystal grain presents the pattern of sheet, and its radical length is 5～15 μ m, and thickness is 0.5～1.0 μ m, and the ratio of width to height is larger, is a kind of desirable template grains.
Claims (3)
1. the preparation method of a sheet bismuth sodium titanate mould plate grain is characterized in that comprising the steps:
(1) adopts molten-salt growth method synthesizing flaky Bi
4Ti
3O
12As presoma;
(2) the sheet presoma that step (1) is synthetic through washing, filtration, oven dry, adds Na
2CO
3, TiO
2Powder is pressed chemical formula Na
0.5Bi
0.5TiO
3Be made into powder, and with etc. the NaCl fused salt of quality in ethanol, mix through ball milling, after the oven dry, be warming up to 1000～1100 ℃ with 3-20 ℃/min, be incubated 1-6 hour;
(3) powder that step (2) is synthetic is through washing, filtration, oven dry.
2. by the preparation method of a kind of sheet bismuth sodium titanate mould plate grain claimed in claim 1, it is characterized in that the total mass of described powder and fused salt and the mass ratio 1: 0.4～0.6 of ethanol.
3. by the preparation method of a kind of sheet bismuth sodium titanate mould plate grain claimed in claim 1, it is characterized in that total mass and the ZrO of described powder and fused salt
2The mass ratio of ball 1: 1～3.
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102211933B (en) * | 2010-11-10 | 2013-07-17 | 中国科学院上海硅酸盐研究所 | Flaky lithium-niobium-titanium (Li-Nb-Ti-O) template grains and preparation method thereof |
| JP6097219B2 (en) * | 2010-11-10 | 2017-03-15 | 中国科学院上海硅酸塩研究所 | Template crystal grains of sheet-like lithium niobate titanate (Li-Nb-Ti-O), textured lithium niobate titanate (Li-Nb-Ti-O) microwave medium ceramics containing the same, and method for producing the same |
| CN102531582B (en) * | 2011-12-29 | 2013-08-21 | 洛阳理工学院 | Method for preparing sodium bismuth titanate nanometer sheet |
| CN103611168A (en) * | 2013-12-02 | 2014-03-05 | 东南大学 | Composite magnetic nanoparticles for targeted therapy of liver cancer and preparation method thereof |
| CN104402432A (en) * | 2014-10-29 | 2015-03-11 | 中南大学 | Textured piezoelectric ceramic material and preparation method thereof |
| CN104986795B (en) * | 2015-07-19 | 2016-09-14 | 北京工业大学 | Under hydrothermal condition, phase separation method obtains Na0.5bi0.5tiO3and the method for Na-Ti-O nano wire |
| CN106946563B (en) * | 2017-04-20 | 2019-05-03 | 成都新柯力化工科技有限公司 | A kind of low cost leadless piezoelectric ceramics and preparation method |
| CN108752010B (en) * | 2018-07-18 | 2021-08-13 | 广东工业大学 | Piezoelectric ceramic, preparation method thereof and 3D printing piezoelectric ceramic device |
| CN111041548B (en) * | 2019-11-21 | 2021-12-17 | 广东工业大学 | Plate-shaped sodium bismuth titanate template crystal grain and preparation method and application thereof |
| CN113501710A (en) * | 2021-06-25 | 2021-10-15 | 淮阴工学院 | Preparation method of sodium bismuth titanate textured ceramic |
| CN114315346A (en) * | 2021-12-10 | 2022-04-12 | 广东华中科技大学工业技术研究院 | Preparation method of large-strain lead-free piezoelectric textured ceramic with double-template texture |
| CN115072773B (en) * | 2022-06-16 | 2023-06-23 | 西安交通大学 | Template for textured lead zirconate titanate-based ceramic and preparation method thereof |
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Application publication date: 20080820 Assignee: SIYANG GRANDE ELECTRONICS Co.,Ltd. Assignor: SHANGHAI INSTITUTE OF CERAMICS, CHINESE ACADEMY OF SCIENCES Contract record no.: X2020320010003 Denomination of invention: Preparation method of sheet bismuth sodium titanate templated grain Granted publication date: 20130116 License type: Exclusive License Record date: 20200312 |
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